JPH0624982B2 - 四塩化ジルコニュウムと四塩化ハフニユウムを分離する方法 - Google Patents
四塩化ジルコニュウムと四塩化ハフニユウムを分離する方法Info
- Publication number
- JPH0624982B2 JPH0624982B2 JP63004416A JP441688A JPH0624982B2 JP H0624982 B2 JPH0624982 B2 JP H0624982B2 JP 63004416 A JP63004416 A JP 63004416A JP 441688 A JP441688 A JP 441688A JP H0624982 B2 JPH0624982 B2 JP H0624982B2
- Authority
- JP
- Japan
- Prior art keywords
- hafnium
- tetrachloride
- zirconium
- zirconium tetrachloride
- low
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 title claims description 78
- PDPJQWYGJJBYLF-UHFFFAOYSA-J hafnium tetrachloride Chemical compound Cl[Hf](Cl)(Cl)Cl PDPJQWYGJJBYLF-UHFFFAOYSA-J 0.000 title claims description 36
- 238000000034 method Methods 0.000 title claims description 11
- 238000005868 electrolysis reaction Methods 0.000 claims description 52
- 229910052735 hafnium Inorganic materials 0.000 claims description 33
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 33
- CSNNHWWHGAXBCP-UHFFFAOYSA-L magnesium sulphate Substances [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 32
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 30
- 150000003839 salts Chemical class 0.000 claims description 15
- PFXYQVJESZAMSV-UHFFFAOYSA-K zirconium(iii) chloride Chemical compound Cl[Zr](Cl)Cl PFXYQVJESZAMSV-UHFFFAOYSA-K 0.000 claims description 8
- -1 hafnium zirconium trichloride Chemical compound 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 3
- 229910001515 alkali metal fluoride Inorganic materials 0.000 claims description 2
- 229910001514 alkali metal chloride Inorganic materials 0.000 claims 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims 1
- 229910001617 alkaline earth metal chloride Inorganic materials 0.000 claims 1
- 150000001342 alkaline earth metals Chemical class 0.000 claims 1
- 230000003247 decreasing effect Effects 0.000 claims 1
- 150000004673 fluoride salts Chemical class 0.000 claims 1
- UJLQXGFCYFUENB-UHFFFAOYSA-J lithium zirconium(4+) tetrachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Zr+4].[Li+] UJLQXGFCYFUENB-UHFFFAOYSA-J 0.000 claims 1
- 239000013589 supplement Substances 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 18
- 239000000460 chlorine Substances 0.000 description 17
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 13
- 229910052726 zirconium Inorganic materials 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 12
- BUKHSQBUKZIMLB-UHFFFAOYSA-L potassium;sodium;dichloride Chemical compound [Na+].[Cl-].[Cl-].[K+] BUKHSQBUKZIMLB-UHFFFAOYSA-L 0.000 description 12
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 11
- 229910007926 ZrCl Inorganic materials 0.000 description 11
- 229910052801 chlorine Inorganic materials 0.000 description 11
- 229910052799 carbon Inorganic materials 0.000 description 9
- 239000007789 gas Substances 0.000 description 9
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 description 5
- 238000004821 distillation Methods 0.000 description 5
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 5
- 229910001928 zirconium oxide Inorganic materials 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- QFFMXYURYVMWLF-UHFFFAOYSA-J [Cl-].[Cl-].[Cl-].[Cl-].[Zr+4].[Hf+4] Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Zr+4].[Hf+4] QFFMXYURYVMWLF-UHFFFAOYSA-J 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 4
- 150000001340 alkali metals Chemical class 0.000 description 4
- 150000001805 chlorine compounds Chemical class 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 3
- 229910003902 SiCl 4 Inorganic materials 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- GJEONJVNTMLKMR-UHFFFAOYSA-K [Cl-].[Cl-].[Cl-].[Hf+3] Chemical compound [Cl-].[Cl-].[Cl-].[Hf+3] GJEONJVNTMLKMR-UHFFFAOYSA-K 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 description 2
- 229910002090 carbon oxide Inorganic materials 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- FGDZQCVHDSGLHJ-UHFFFAOYSA-M rubidium chloride Chemical compound [Cl-].[Rb+] FGDZQCVHDSGLHJ-UHFFFAOYSA-M 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000010517 secondary reaction Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 229910016036 BaF 2 Inorganic materials 0.000 description 1
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- GEIAQOFPUVMAGM-UHFFFAOYSA-N ZrO Inorganic materials [Zr]=O GEIAQOFPUVMAGM-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 229910000449 hafnium oxide Inorganic materials 0.000 description 1
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 229910052914 metal silicate Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/04—Halides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G27/00—Compounds of hafnium
- C01G27/04—Halides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Electrolytic Production Of Metals (AREA)
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63004416A JPH0624982B2 (ja) | 1988-01-12 | 1988-01-12 | 四塩化ジルコニュウムと四塩化ハフニユウムを分離する方法 |
| CA000587064A CA1333781C (fr) | 1988-01-12 | 1988-12-28 | Procede pour la separation du tetrachlorure d'hafnium du tetrachlorure de zirconium |
| US07/293,791 US5009751A (en) | 1988-01-12 | 1989-01-05 | Process for separation of hafnium tetrachloride from zirconium tetrachloride |
| AU28322/89A AU612452B2 (en) | 1988-01-12 | 1989-01-09 | A process for separation of hafnium tetrachloride from zirconium tetrachloride |
| FR898900263A FR2625739B1 (fr) | 1988-01-12 | 1989-01-11 | Procede de separation du tetrachlorure de hafnium d'avec du tetrachlorure de zirconium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63004416A JPH0624982B2 (ja) | 1988-01-12 | 1988-01-12 | 四塩化ジルコニュウムと四塩化ハフニユウムを分離する方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01179726A JPH01179726A (ja) | 1989-07-17 |
| JPH0624982B2 true JPH0624982B2 (ja) | 1994-04-06 |
Family
ID=11583689
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63004416A Expired - Lifetime JPH0624982B2 (ja) | 1988-01-12 | 1988-01-12 | 四塩化ジルコニュウムと四塩化ハフニユウムを分離する方法 |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US5009751A (fr) |
| JP (1) | JPH0624982B2 (fr) |
| AU (1) | AU612452B2 (fr) |
| CA (1) | CA1333781C (fr) |
| FR (1) | FR2625739B1 (fr) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06104912B2 (ja) * | 1988-04-01 | 1994-12-21 | 三菱原子燃料株式会社 | 四塩化ジルコニユウムと四塩化ハフニユウムを分離する方法及び電極 |
| US4874475A (en) * | 1988-09-12 | 1989-10-17 | Westinghouse Electric Corp. | Molten salt extractive distillation process for zirconium-hafnium separation |
| FR2823740B1 (fr) * | 2001-04-18 | 2004-02-06 | Cezus Co Europ Zirconium | Procede de separation des tetrachlorures de zirconium et de hafnium |
| US20060062910A1 (en) * | 2004-03-01 | 2006-03-23 | Meiere Scott H | Low zirconium, hafnium-containing compositions, processes for the preparation thereof and methods of use thereof |
| US20050214458A1 (en) * | 2004-03-01 | 2005-09-29 | Meiere Scott H | Low zirconium hafnium halide compositions |
| FR2876369B1 (fr) * | 2004-10-11 | 2006-12-22 | Cie Europ Du Zirconium Cezus S | Procede de separation du zirconium et du hafnium |
| CN111041512A (zh) * | 2019-12-25 | 2020-04-21 | 中国科学院高能物理研究所 | 一种变价金属的低价卤化物的制备方法 |
| CN111249761B (zh) * | 2020-03-04 | 2022-01-28 | 中国科学院上海应用物理研究所 | 一种熔盐蒸馏纯化方法及设备 |
| CN116750793A (zh) * | 2023-07-07 | 2023-09-15 | 朝阳东锆新材料有限公司 | 一种生产精四氯化锆的方法 |
Family Cites Families (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA627327A (en) * | 1961-09-12 | W. Ancrum Robert | Production of metallic halides | |
| CA611153A (en) * | 1960-12-20 | W. Ancrum Robert | Electrolytic preparation of titanium tetrahalides | |
| US679997A (en) * | 1898-11-14 | 1901-08-06 | Charles W Roepper | Electrolytic process of obtaining metals from their fused compounds. |
| GB708595A (en) * | 1951-06-12 | 1954-05-05 | Titan Co Inc | A method and apparatus for the purification of titanium tetrachloride |
| US2791485A (en) * | 1952-12-03 | 1957-05-07 | Commw Scient Ind Res Org | Process for removal of hafnium from zirconium-containing material |
| US2894886A (en) * | 1954-07-16 | 1959-07-14 | Horizons Titanium Corp | Fused salt bath for electrodeposition of transition metals |
| US2961293A (en) * | 1957-02-19 | 1960-11-22 | Mallory Sharon Metals Corp | Purification of hafnium tetrahalide |
| US3734689A (en) * | 1969-02-07 | 1973-05-22 | Wisconsin Alumni Res Found | Process for separation of hafnium from zirconium |
| US3600284A (en) * | 1969-02-18 | 1971-08-17 | Us Interior | Method of adding refractory metal halides to molten salt electrolytes |
| US3856477A (en) * | 1970-12-28 | 1974-12-24 | H Ishizuka | Process for refining zirconium tetrachloride containing hafnium tetrachloride |
| US3725221A (en) * | 1972-01-26 | 1973-04-03 | M Wong | Recovery of niobium and tantalum |
| FR2494727A1 (fr) * | 1980-11-27 | 1982-05-28 | Armand Marcel | Cellule pour la preparation de metaux polyvalents tels que zr ou hf par electrolyse d'halogenures fondus et procede de mise en oeuvre de cette cellule |
| JPS6044119A (ja) * | 1983-08-19 | 1985-03-09 | Sumitomo Metal Ind Ltd | 可動スリ−ブ式圧延ロ−ルのスリ−ブ移動装置 |
| FR2560896B1 (fr) * | 1984-03-12 | 1989-10-20 | Pechiney | Procede d'obtention d'un metal par electrolyse d'halogenures en bain de sels fondus comportant un double depot simultane et continu et dispositifs d'application |
| US4578252A (en) * | 1985-05-14 | 1986-03-25 | Hughes Aircraft Company | Method for preparing ultra-pure zirconium and hafnium tetrafluorides |
| JPH0633476B2 (ja) * | 1987-05-27 | 1994-05-02 | 三菱原子燃料株式会社 | 融解塩電解によるジルコニユウムとハフニユウムの分離方法 |
| JPH06104912B2 (ja) * | 1988-04-01 | 1994-12-21 | 三菱原子燃料株式会社 | 四塩化ジルコニユウムと四塩化ハフニユウムを分離する方法及び電極 |
| US4874475A (en) * | 1988-09-12 | 1989-10-17 | Westinghouse Electric Corp. | Molten salt extractive distillation process for zirconium-hafnium separation |
| US4865695A (en) * | 1988-09-12 | 1989-09-12 | Westinghouse Electric Corp. | Preparation of complexes of zirconium and hafnium tetrachlorides with phosphorus oxychloride |
-
1988
- 1988-01-12 JP JP63004416A patent/JPH0624982B2/ja not_active Expired - Lifetime
- 1988-12-28 CA CA000587064A patent/CA1333781C/fr not_active Expired - Fee Related
-
1989
- 1989-01-05 US US07/293,791 patent/US5009751A/en not_active Expired - Fee Related
- 1989-01-09 AU AU28322/89A patent/AU612452B2/en not_active Ceased
- 1989-01-11 FR FR898900263A patent/FR2625739B1/fr not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| FR2625739A1 (fr) | 1989-07-13 |
| US5009751A (en) | 1991-04-23 |
| CA1333781C (fr) | 1995-01-03 |
| AU2832289A (en) | 1989-07-13 |
| AU612452B2 (en) | 1991-07-11 |
| JPH01179726A (ja) | 1989-07-17 |
| FR2625739B1 (fr) | 1991-10-25 |
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